WO2020158907A1 - グリース組成物 - Google Patents

グリース組成物 Download PDF

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Publication number
WO2020158907A1
WO2020158907A1 PCT/JP2020/003580 JP2020003580W WO2020158907A1 WO 2020158907 A1 WO2020158907 A1 WO 2020158907A1 JP 2020003580 W JP2020003580 W JP 2020003580W WO 2020158907 A1 WO2020158907 A1 WO 2020158907A1
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Prior art keywords
grease composition
grease
group
bearing
urea
Prior art date
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PCT/JP2020/003580
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English (en)
French (fr)
Japanese (ja)
Inventor
孝仁 高根
渡邊　剛
昭弘 宍倉
山下　潤
Original Assignee
出光興産株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 出光興産株式会社 filed Critical 出光興産株式会社
Priority to EP20749088.9A priority Critical patent/EP3919592A4/en
Priority to JP2020568622A priority patent/JPWO2020158907A1/ja
Priority to US17/423,252 priority patent/US11746303B2/en
Priority to CN202080011236.9A priority patent/CN113348234B/zh
Publication of WO2020158907A1 publication Critical patent/WO2020158907A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/045—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/02—Petroleum fractions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/02—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/68—Esters
    • C10M129/74—Esters of polyhydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/04—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M133/12—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to a carbon atom of a six-membered aromatic ring
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/06—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic nitrogen-containing compound
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/02—Mixtures of base-materials and thickeners
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C33/00—Parts of bearings; Special methods for making bearings or parts thereof
    • F16C33/30—Parts of ball or roller bearings
    • F16C33/66—Special parts or details in view of lubrication
    • F16C33/6603—Special parts or details in view of lubrication with grease as lubricant
    • F16C33/6633—Grease properties or compositions, e.g. rheological properties
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/003—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
    • C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/283—Esters of polyhydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • C10M2215/1026—Ureas; Semicarbazides; Allophanates used as thickening material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/26—Amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/02—Viscosity; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02—Pour-point; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C2210/00—Fluids
    • F16C2210/02—Fluids defined by their properties
    • F16C2210/04—Fluids defined by their properties by viscosity
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C2240/00—Specified values or numerical ranges of parameters; Relations between them
    • F16C2240/26—Speed, e.g. rotational speed
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C2300/00—Application independent of particular apparatuses
    • F16C2300/20—Application independent of particular apparatuses related to type of movement
    • F16C2300/22—High-speed rotation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C33/00—Parts of bearings; Special methods for making bearings or parts thereof
    • F16C33/02—Parts of sliding-contact bearings
    • F16C33/04—Brasses; Bushes; Linings
    • F16C33/06—Sliding surface mainly made of metal
    • F16C33/10—Construction relative to lubrication
    • F16C33/102—Construction relative to lubrication with grease as lubricant

Definitions

  • the present invention relates to a grease composition.
  • Grease is a semi-solid lubricant containing a base oil and a thickener.
  • grease using lithium soap as a thickener (hereinafter, also referred to as “lithium soap grease”) is used for automobiles, machine tools, It is also widely used in bearings for construction machinery.
  • a grease using a urea thickener (hereinafter, also referred to as “urea grease”) is known as a grease having a long lubricating life at high temperature and excellent in oxidation stability, heat resistance, and water resistance. (For example, refer to Patent Document 1).
  • An object of the present invention is to provide a grease composition capable of imparting excellent durability to a bearing used under a high speed rotation condition with a DN value of 100,000 or more.
  • the “DN value” means the product of D and N when the inner diameter of the bearing is D (unit: mm) and the rotation speed of the bearing is N (rpm).
  • the present inventors paid attention to the particle size of the particles containing the urea-based thickener in the grease composition. Then, it was found that a grease composition in which the arithmetic mean particle diameter on an area basis when the particles are measured by a laser diffraction/scattering method is adjusted to a predetermined range can solve the above problems, and the present invention is completed.
  • a grease composition containing a base oil (A) and a urea thickener (B), Particles containing the urea thickener (B) in the grease composition satisfy the following requirement (I), Requirement (I):
  • the area-based arithmetic average particle diameter of the particles is 2.0 ⁇ m or less when the particles are measured by a laser diffraction/scattering method.
  • the grease composition according to [1], wherein the particles containing the urea thickener (B) in the grease composition further satisfy the following requirement (II).
  • the specific surface area of the particles measured by a laser diffraction/scattering method is 20,000 cm 2 /cm 3 or more.
  • the base oil (A) is one or more selected from mineral oils, hydrocarbon-based oils, aromatic-based oils, ester-based oils, and ether-based oils, and described in [1] or [2].
  • Grease composition [4] The grease composition according to any one of [1] to [3], wherein the base oil (A) has a kinematic viscosity at 40° C. of 10 to 300 mm 2 /s.
  • R 3 represents a divalent aromatic hydrocarbon group having 6 to 18 carbon atoms.
  • the grease composition according to claim 1 A bearing that is lubricated with the grease composition according to any one of the above [1] to [9] and that is used under high speed rotation conditions with a DN value of 100,000 or more. [11] A lubrication method in which the grease composition according to any one of [1] to [9] is used to lubricate a bearing used under a high speed rotation condition with a DN value of 100,000 or more.
  • the grease composition of the present invention contains a base oil (A) and a urea thickener (B).
  • base oil (A) and the “urea thickener (B)” are also referred to as “component (A)” and “component (B)", respectively.
  • the total content of components (A) and (B) is preferably 60% by mass or more, more preferably 70% by mass based on the total amount (100% by mass) of the grease composition. To 100% by mass, more preferably 80 to 100% by mass, still more preferably 90 to 100% by mass.
  • the grease composition of one aspect of the present invention may contain components other than the components (A) and (B) as long as the effects of the present invention are not impaired.
  • particles containing the urea thickener (B) in the grease composition satisfy the following requirement (I).
  • the requirement (I) is a parameter indicating the state of aggregation of the urea thickener (B) in the grease composition.
  • the "particles containing the urea thickener (B) to be measured by the laser diffraction/scattering method” means particles formed by agglomeration of the urea thickener (B) contained in the grease composition. Refers to.
  • the particle size defined by the above requirement (I) is a grease prepared under the same conditions without blending the additive. It can be obtained by measuring the composition by a laser diffraction/scattering method.
  • the additive is liquid at room temperature (25° C.)
  • the grease composition containing the additive may be a measurement target.
  • the urea-based thickener (B) is usually obtained by reacting an isocyanate compound with a monoamine, but since the reaction speed is very fast, the urea-based thickener (B) aggregates to form large particles ( Micelle particles, so-called “damage”) are likely to occur excessively.
  • the particle diameter defined by the above requirement (I) exceeds 2.0 ⁇ m, the DN value has excellent durability against a bearing used under high speed rotation conditions of 100,000 or more. It has been found that it is difficult to impart sex.
  • the particle size defined by the above requirement (I) finer to 2.0 ⁇ m or less, the retention of the base oil (A) by the particles is improved and the fluidity of the grease composition itself is also improved. Therefore, even under the condition where the bearing rotates at high speed, the particles satisfactorily retain the base oil (A), the grease composition satisfactorily spreads over a portion requiring lubrication, and the DN value is 100,000 or more under high-speed rotation conditions. It is presumed that it is possible to impart excellent durability to the bearing used in.
  • the particle size defined by the above requirement (I) is preferably 1.5 ⁇ m or less, more preferably 1.0 ⁇ m or less, still more preferably 0.9 ⁇ m or less, It is more preferably 0.8 ⁇ m or less, still more preferably 0.7 ⁇ m or less, and further preferably 0.6 ⁇ m or less. Further, it is usually 0.01 ⁇ m or more.
  • the grease composition of one aspect of the present invention preferably further satisfies the following requirement (II).
  • the specific surface area of the particles measured by a laser diffraction/scattering method is 20,000 cm 2 /cm 3 or more.
  • the specific surface area defined by the above requirement (II) is a secondary index showing the state of fineness of the particles containing the urea thickener (B) in the grease composition and the presence of large particles (damage). is there. That is, by satisfying the above requirement (I) and further satisfying the above requirement (II), the state of micronization of the particles containing the urea thickener (B) in the grease composition is better, and large particles can be obtained.
  • the existence of (damage) is also suppressed. Therefore, it becomes easier to impart excellent durability to a bearing used under a high-speed rotation condition with a DN value of 100,000 or more.
  • the specific surface area defined by the requirement (II) is preferably 50,000 cm 2 /cm 3 or more, more preferably 100,000 cm 2 /cm 3 or more, and further preferably 200,000 cm 2 /cm 3 or more. Is.
  • the values defined by the requirement (I) and further the requirement (II) are values measured by the method described in Examples described later. Further, the values defined by the above requirement (I) and further the above requirement (II) can be adjusted mainly by the production conditions of the urea thickener (B).
  • the details of each component contained in the grease composition of the present invention will be described, focusing on the specific means for adjusting the value defined by the requirement (I) and the requirement (II).
  • the base oil (A) contained in the grease composition of the present invention may be any base oil generally used in grease compositions, and examples thereof include one or more selected from mineral oils and synthetic oils.
  • Examples of the mineral oil include paraffin crude oil, intermediate base crude oil, or distillate oil obtained by distilling naphthene crude oil under atmospheric pressure or reduced pressure, and refined oil obtained by refining these distillate oils.
  • Examples of the refining method for obtaining a refined oil include hydroreforming treatment, solvent extraction treatment, solvent dewaxing treatment, hydroisomerization dewaxing treatment, hydrofinishing treatment, and clay treatment.
  • synthetic oils examples include hydrocarbon oils, aromatic oils, ester oils, and ether oils. Further, a synthetic oil obtained by isomerizing a wax (GTL wax) produced by the Fischer-Tropsch method or the like can also be mentioned.
  • hydrocarbon oil examples include normal paraffin, isoparaffin, polybutene, polyisobutylene, 1-decene oligomer, poly- ⁇ -olefins (PAO) such as 1-decene and ethylene cooligomers, and hydrides thereof. ..
  • aromatic oil examples include alkylbenzene such as monoalkylbenzene and dialkylbenzene; alkylnaphthalene such as monoalkylnaphthalene, dialkylnaphthalene and polyalkylnaphthalene; and the like.
  • ester oil examples include dibutyl sebacate, di-2-ethylhexyl sebacate, dioctyl adipate, diisodecyl adipate, ditridecyl adipate, ditridecyl glutarate, and methylacetylricinoleate; trioctyl trimellitate, trioctyl trimellitate Aromatic ester oils such as decyl trimellitate and tetraoctyl pyromellitate; polyol esters such as trimethylol propane caprylate, trimethylol propane belargonate, pentaerythritol-2-ethylhexanoate, pentaerythritol belargonate Oils; complex ester oils such as oligoesters of polyhydric alcohols and mixed fatty acids of dibasic acids and monobasic acids; and the like.
  • ether oils include polyglycols such as polyethylene glycol, polypropylene glycol, polyethylene glycol monoether and polypropylene glycol monoether; monoalkyl triphenyl ethers, alkyldiphenyl ethers, dialkyldiphenyl ethers, pentaphenyl ethers, tetraphenyl ethers, monoalkyls. Phenyl ether oils such as tetraphenyl ether and dialkyl tetraphenyl ether; and the like.
  • the base oil (A) is preferably a synthetic oil, more preferably a hydrocarbon-based oil, an ester-based oil, and an ether-based oil when oxidative stability at high temperatures is required. Also, by using a mixture of hydrocarbon-based oil, ester-based oil, and ether-based oil, it is possible to balance heat resistance, seal resistance, and low temperature characteristics.
  • the base oil (A) used in one embodiment of the present invention has a kinematic viscosity at 40° C. of preferably 10 to 300 mm 2 /s, more preferably 15 to 200 mm 2 /s, still more preferably 20 to 150 mm 2 /s. is there.
  • the base oil (A) used in one embodiment of the present invention may be a mixed base oil prepared by combining a high-viscosity base oil and a low-viscosity base oil to adjust the kinematic viscosity to the above range.
  • the viscosity index of the base oil (A) used in one embodiment of the present invention is preferably 60 or more, more preferably 70 or more, and further preferably 80 or more.
  • the kinematic viscosity and the viscosity index mean values measured or calculated according to JIS K2283:2000.
  • the content of the base oil (A) is preferably 50% by mass or more, more preferably 55% by mass or more, based on the total amount (100% by mass) of the grease composition. More preferably 60 mass% or more, still more preferably 65 mass% or more, preferably 98.5 mass% or less, more preferably 97 mass% or less, further preferably 95 mass% or less, even more preferably It is 93 mass% or less.
  • the urea-based thickener (B) contained in the grease composition of the present invention may be a compound having a urea bond, but a diurea compound having two urea bonds is preferable and represented by the following general formula (b1).
  • the diurea compound to be used is more preferable.
  • the urea thickener (B) used in one embodiment of the present invention may be composed of one kind or may be a mixture of two or more kinds.
  • R 1 and R 2 each independently represent a monovalent hydrocarbon group having 6 to 24 carbon atoms.
  • R 1 and R 2 may be the same or different from each other.
  • R 3 represents a divalent aromatic hydrocarbon group having 6 to 18 carbon atoms.
  • the monovalent hydrocarbon group that can be selected as R 1 and R 2 in the general formula (b1) has 6 to 24 carbon atoms, preferably 6 to 20 carbon atoms, and more preferably 6 to 18 carbon atoms. ..
  • a saturated or unsaturated monovalent chain hydrocarbon group a saturated or unsaturated monovalent alicyclic hydrocarbon group, 1 A valent aromatic hydrocarbon group may be mentioned.
  • the content of the chain hydrocarbon group is X molar equivalent
  • the content of the alicyclic hydrocarbon group is Y molar equivalent
  • the aromatic hydrocarbon When the content of the group is Z molar equivalent, it is preferable that the following requirements (a) and (b) are satisfied.
  • Requirement (b): X/Y ratio is 0 to 100 (preferably 10/90 to 90/10, more preferably 20/80 to 85/15, and further preferably 40/60 to 85/15).
  • the alicyclic hydrocarbon group, the chain hydrocarbon group, and the aromatic hydrocarbon group are groups selected as R 1 and R 2 in the general formula (b1)
  • X The sum of the values of Y, Y, and Z is 2 molar equivalents with respect to 1 mole of the compound represented by the general formula (b1).
  • the values of the requirements (a) and (b) mean the average value with respect to the total amount of the compound group represented by the general formula (b1) contained in the grease composition.
  • the compound represented by the general formula (b1) which satisfies the above requirements (a) and (b)
  • both the lubricating life and the lubricating performance of the grease composition are compatible, and the DN value is 100,000 or more. It is easy to give excellent durability to bearings used under high speed rotation conditions.
  • the values of X, Y, and Z can be calculated from the molar equivalent of each amine used as a raw material.
  • Examples of the monovalent saturated chain hydrocarbon group include a straight chain or branched chain alkyl group having 6 to 24 carbon atoms, specifically, a hexyl group, a heptyl group, an octyl group, a nonyl group, a decyl group, Examples thereof include undecyl group, dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, hexadecyl group, heptadecyl group, octadecyl group, nonadecyl group and icosyl group.
  • a linear or branched alkyl group having 10 to 20 carbon atoms is preferable, and a linear or branched alkyl group having 16 to 20 carbon atoms is more preferable. Further, the alkyl group is preferably linear.
  • the monovalent unsaturated chain hydrocarbon group include a straight chain or branched chain alkenyl group having 6 to 24 carbon atoms, and specific examples thereof include a hexenyl group, a heptenyl group, an octenyl group, a nonenyl group and a decenyl group.
  • the monovalent saturated chain hydrocarbon group and the monovalent unsaturated chain hydrocarbon group may be linear or branched. Among these, a linear or branched alkenyl group having 10 to 20 carbon atoms is preferable, and a linear or branched alkenyl group having 16 to 20 carbon atoms is more preferable. Further, the alkenyl group is preferably linear.
  • Examples of the monovalent saturated alicyclic hydrocarbon group include cycloalkyl groups such as cyclohexyl group, cycloheptyl group, cyclooctyl group and cyclononyl group; methylcyclohexyl group, dimethylcyclohexyl group, ethylcyclohexyl group, diethylcyclohexyl group, Cycloalkyl group substituted with an alkyl group having 1 to 6 carbon atoms such as propylcyclohexyl group, isopropylcyclohexyl group, 1-methyl-propylcyclohexyl group, butylcyclohexyl group, pentylcyclohexyl group, pentyl-methylcyclohexyl group, hexylcyclohexyl group (Preferably a cyclohexyl group substituted with an alkyl group having 1 to 6 carbon atoms); and the like.
  • Examples of the monovalent unsaturated alicyclic hydrocarbon group include cycloalkenyl groups such as cyclohexenyl group, cycloheptenyl group, and cyclooctenyl group; methylcyclohexenyl group, dimethylcyclohexenyl group, ethylcyclohexenyl group, diethylcyclohexenyl group.
  • a cycloalkenyl group substituted with an alkyl group having 1 to 6 carbon atoms such as a propylcyclohexenyl group (preferably a cyclohexenyl group substituted with an alkyl group having 1 to 6 carbon atoms); and the like.
  • Examples of the monovalent aromatic hydrocarbon group include phenyl group, biphenyl group, terphenyl group, naphthyl group, diphenylmethyl group, diphenylethyl group, diphenylpropyl group, methylphenyl group, dimethylphenyl group, ethylphenyl group, Examples include propylphenyl group.
  • the divalent aromatic hydrocarbon group that can be selected as R 3 in the general formula (b1) has 6 to 18 carbon atoms, preferably 6 to 15 carbon atoms, and more preferably 6 to 13 carbon atoms.
  • Examples of the divalent aromatic hydrocarbon group that can be selected as R 3 include a phenylene group, a diphenylmethylene group, a diphenylethylene group, a diphenylpropylene group, a methylphenylene group, a dimethylphenylene group, and an ethylphenylene group.
  • a phenylene group, a diphenylmethylene group, a diphenylethylene group, or a diphenylpropylene group is preferable, and a diphenylmethylene group is more preferable.
  • the content of the component (B) is preferably 1 to 40% by mass, more preferably 2 to 30% by mass, based on the total amount (100% by mass) of the grease composition. %, more preferably 4 to 25% by mass, even more preferably 6 to 20% by mass, still more preferably 9 to 18% by mass. If the amount of the thickener is too large, it becomes hard and the lubricity becomes poor. On the other hand, if the amount of the thickener becomes too small, a problem of leakage at high speed rotation may occur. When the content of the component (B) is 1% by mass or more, it is easy to adjust the blending consistency of the resulting grease composition to an appropriate range. On the other hand, when the content of the component (B) is 40% by mass or less, the obtained grease composition does not become too hard and is excellent for a bearing used under a high speed rotation condition with a DN value of 100,000 or more. It becomes easy to add durability.
  • the urea thickener (B) can be usually obtained by reacting an isocyanate compound with a monoamine.
  • the reaction is preferably carried out by adding the solution ⁇ prepared by dissolving the monoamine in the base oil (A) to the heated solution ⁇ obtained by dissolving the isocyanate compound in the base oil (A).
  • the isocyanate compound may be a group corresponding to the divalent aromatic hydrocarbon group represented by R 3 in the general formula (b1).
  • the desired urea-based thickener (B) is obtained by the above-mentioned method using the diisocyanate having the same and the amine having the group corresponding to the monovalent hydrocarbon group represented by R 1 and R 2 as the monoamine. Can be synthesized.
  • the grease production as shown in the following [1] It is preferable to manufacture the grease composition containing the component (A) and the component (B) using an apparatus.
  • a container body having an introduction part for introducing a grease raw material and a discharge part for discharging grease to the outside, Having a rotation axis in the axial direction of the inner circumference of the container body, and comprising a rotor rotatably provided inside the container body,
  • the rotor is (I) The unevenness is alternately provided along the surface of the rotor, and the unevenness is inclined with respect to the rotation axis, (Ii)
  • a grease manufacturing apparatus including a first uneven portion having a feeding ability from the introduction portion toward the discharge portion.
  • FIG. 1 is a schematic cross-sectional view of the grease manufacturing apparatus of the above [1] that can be used in one embodiment of the present invention.
  • the grease manufacturing apparatus 1 shown in FIG. 1 has a container body 2 into which a grease raw material is introduced, and a rotary shaft 12 on the central axis of the inner circumference of the container main body 2, and the rotary shaft 12 rotates about the central axis.
  • a child 3 The rotor 3 rotates at high speed around the rotation shaft 12 as a central axis, and gives a high shearing force to the grease raw material inside the container body 2. As a result, a grease containing the urea thickener is produced. As shown in FIG.
  • the container body 2 may be partitioned into an introduction part 4, a retention part 5, a first inner peripheral surface 6, a second inner peripheral surface 7, and a discharge part 8 in order from the upstream side.
  • the container body 2 preferably has a frustoconical inner peripheral surface whose inner diameter gradually increases from the introducing portion 4 toward the discharging portion 8.
  • the introduction part 4 which is one end of the container body 2 includes a plurality of solution introduction tubes 4A and 4B for introducing the grease raw material from the outside of the container body 2.
  • the retention part 5 is a space that is arranged downstream of the introduction part 4 and temporarily retains the grease raw material introduced from the introduction part 4.
  • the grease attached to the inner peripheral surface of the staying portion 5 forms a large lump, so that the grease is transported to the first inner circumferential surface 6 on the downstream side in the shortest possible time.
  • the first inner peripheral surface 6 is arranged in the downstream portion adjacent to the retention portion 5, and the second inner peripheral surface 7 is arranged in the downstream portion adjacent to the first inner peripheral surface 6.
  • the provision of the first uneven portion 9 on the first inner peripheral surface 6 and the provision of the second uneven portion 10 on the second inner peripheral surface 7 mean that the first inner peripheral surface 6 and the second inner peripheral surface 6 are provided. It is preferable in that the peripheral surface 7 functions as a high-shear portion that applies a high shear force to the grease raw material or the grease.
  • the discharge part 8 which is the other end of the container body 2 is a part which discharges the grease agitated by the first inner peripheral surface 6 and the second inner peripheral surface 7, and has a discharge port 11 for discharging the grease.
  • the discharge port 11 is formed in a direction orthogonal to the rotation shaft 12 or in a direction substantially orthogonal thereto.
  • the grease is discharged from the discharge port 11 in a direction orthogonal to the rotation shaft 12 or in a direction substantially orthogonal thereto.
  • the discharge port 11 does not necessarily need to be orthogonal to the rotation shaft 12, and may be formed in a direction parallel or substantially parallel to the rotation shaft 12.
  • the rotor 3 is rotatably provided with the central axis of the frustoconical inner peripheral surface of the container body 2 as the rotation axis 12, and when the container body 2 is viewed from the upstream portion to the downstream portion as shown in FIG. Then, rotate counterclockwise.
  • the rotor 3 has an outer peripheral surface that expands in accordance with an increase in the inner diameter of the truncated cone of the container body 2, and the outer peripheral surface of the rotor 3 and the inner peripheral surface of the truncated cone of the container body 2 have a constant distance. Has been maintained.
  • the outer peripheral surface of the rotor 3 is provided with a first concavo-convex portion 13 of the rotor in which irregularities are alternately provided along the surface of the rotor 3.
  • the first concavo-convex portion 13 of the rotor is inclined from the introduction portion 4 toward the discharge portion 8 with respect to the rotation shaft 12 of the rotor 3, and has a feeding ability from the introduction portion 4 toward the discharge portion 8 direction. That is, the first concavo-convex portion 13 of the rotor is inclined in the direction in which the solution is pushed to the downstream side when the rotor 3 rotates in the direction shown in FIG.
  • the step between the concave portion 13A and the convex portion 13B of the first concavo-convex portion 13 of the rotor is preferably 0.3 to 30, and more preferably 0.5, when the diameter of the concave portion 13A of the outer peripheral surface of the rotor 3 is 100. -15, more preferably 2-7.
  • the number of the convex portions 13B of the first concave-convex portion 13 of the rotor in the circumferential direction is preferably 2 to 1000, more preferably 6 to 500, and further preferably 12 to 200.
  • the ratio of the width of the convex portion 13B of the first concave-convex portion 13 of the rotor to the width of the concave portion 13A [width of convex portion/width of concave portion] in a cross section orthogonal to the rotation axis 12 of the rotor 3 is preferably 0. 0.01 to 100, more preferably 0.1 to 10, and still more preferably 0.5 to 2.
  • the inclination angle of the first concavo-convex portion 13 of the rotor with respect to the rotating shaft 12 is preferably 2 to 85 degrees, more preferably 3 to 45 degrees, and further preferably 5 to 20 degrees.
  • the first inner peripheral surface 6 of the container body 2 is provided with a first concavo-convex portion 9 having a plurality of concavities and convexities formed along the inner peripheral surface. Further, it is preferable that the unevenness of the first uneven portion 9 on the container body 2 side is inclined in the opposite direction to the first uneven portion 13 of the rotor. That is, the plurality of concavities and convexities of the first concavo-convex portion 9 on the container body 2 side should be inclined in the direction of pushing the solution downstream when the rotation shaft 12 of the rotor 3 rotates in the direction shown in FIG. Is preferred.
  • the first unevenness portion 9 having a plurality of unevennesses provided on the first inner circumferential surface 6 of the container body 2 further enhances the stirring ability and the discharge ability.
  • the depth of the unevenness of the first uneven portion 9 on the container body 2 side is preferably 0.2 to 30, more preferably 0.5 to 15, and further preferably 1 to 1, when the inner diameter (diameter) of the container is 100. It is 5.
  • the number of the irregularities of the first irregularity portion 9 on the container body 2 side is preferably 2 to 1000, more preferably 6 to 500, and further preferably 12 to 200.
  • the ratio of the width of the concave portion of the first concave-convex portion 9 on the container body 2 side to the width of the convex portion between the grooves [the width of the concave portion/the width of the convex portion] is preferably 0.01 to 100, more preferably Is 0.1 to 10, more preferably 0.5 to 2 or less.
  • the inclination angle of the unevenness of the first uneven portion 9 on the container body 2 side with respect to the rotating shaft 12 is preferably 2 to 85 degrees, more preferably 3 to 45 degrees, and further preferably 5 to 20 degrees.
  • the first inner peripheral surface 6 of the container body 2 is provided with the first concave-convex portion 9, the first inner peripheral surface 6 can function as a shearing portion that imparts a high shearing force to the grease raw material or the grease.
  • the first uneven portion 9 does not necessarily have to be provided.
  • the second concavo-convex portion 14 of the rotor On the outer peripheral surface of the downstream portion of the first concavo-convex portion 13 of the rotor, it is preferable that the second concavo-convex portion 14 of the rotor, in which irregularities are alternately provided, is provided along the surface of the rotor 3.
  • the second concavo-convex portion 14 of the rotor is inclined with respect to the rotation shaft 12 of the rotor 3 and has a feed suppressing ability that pushes the solution back to the upstream side from the introducing portion 4 toward the discharging portion 8.
  • the step difference of the second concave-convex portion 14 of the rotor is preferably 0.3 to 30, more preferably 0.5 to 15, and further preferably 2 to 7 when the diameter of the concave portion of the outer peripheral surface of the rotor 3 is 100. Is.
  • the number of convex portions of the second concave-convex portion 14 of the rotor in the circumferential direction is preferably 2 to 1000, more preferably 6 to 500, and further preferably 12 to 200.
  • the ratio of the width of the convex portion of the second concave-convex portion 14 of the rotor to the width of the concave portion in the cross section orthogonal to the rotation axis of the rotor 3 [width of convex portion/width of concave portion] is preferably 0.01 to 100, more preferably 0.1 to 10, and still more preferably 0.5 to 2.
  • the inclination angle of the second concavo-convex portion 14 of the rotor with respect to the rotating shaft 12 is preferably 2 to 85 degrees, more preferably 3 to 45 degrees, and further preferably 5 to 20 degrees.
  • the second inner peripheral surface 7 of the container body 2 is provided with a second concavo-convex portion 10 adjacent to a downstream portion of the concavo-convex portion of the first concavo-convex portion 9 on the container body 2 side and having a plurality of concavo-convex portions formed therein. It is preferable. It is preferable that a plurality of irregularities be formed on the inner peripheral surface of the container body 2, and that each irregularity be inclined in the opposite direction to the inclination direction of the second irregularity portion 14 of the rotor.
  • the plurality of concavities and convexities of the second concavo-convex portion 10 on the container body 2 side are inclined in a direction in which the solution is pushed back to the upstream side when the rotating shaft 12 of the rotor 3 rotates in the direction shown in FIG. Is preferred.
  • the stirring ability is further enhanced by the unevenness of the second uneven portion 10 provided on the second inner peripheral surface 7 of the container body 2.
  • the second inner peripheral surface 7 of the container body can be made to function as a shearing portion that applies a high shearing force to the grease raw material or the grease.
  • the depth of the concave portion of the second uneven portion 10 on the container body 2 side is preferably 0.2 to 30, more preferably 0.5 to 15, and further preferably, when the inner diameter (diameter) of the container body 2 is 100. Is 1 to 5.
  • the number of recesses of the second uneven portion 10 on the container body 2 side is preferably 2 to 1000, more preferably 6 to 500, and further preferably 12 to 200.
  • the ratio of the width of the convex portion of the concave and convex of the second concave and convex portion 10 on the container body 2 side to the width of the concave portion in the cross section orthogonal to the rotation axis 12 of the rotor 3 [width of convex portion/width of concave portion] is preferably Is 0.01 to 100, more preferably 0.1 to 10, and still more preferably 0.5 to 2 or less.
  • the inclination angle of the second uneven portion 10 on the container body 2 side with respect to the rotation axis 12 is preferably 2 to 85 degrees, more preferably 3 to 45 degrees, and further preferably 5 to 20 degrees.
  • the ratio of the length of the first uneven portion 9 on the container body 2 side to the length of the second uneven portion 10 on the container body 2 side [length of the first uneven portion/length of the second uneven portion] is preferably It is 2/1 to 20/1.
  • FIG. 2 is a cross-sectional view of the first uneven portion 9 on the container body 2 side of the grease manufacturing apparatus 1 in a direction orthogonal to the rotation axis 12.
  • a plurality of scrapers 15 are provided on the first concave-convex portion 13 of the rotor shown in FIG. Has been.
  • the second uneven portion 14 is also provided with a plurality of scrapers in which the tip of the convex portion projects toward the inner peripheral surface side of the container body 2 as in the case of the first uneven portion 13.
  • the scraper 15 scrapes off the grease attached to the inner peripheral surfaces of the first uneven portion 9 on the container body 2 side and the second uneven portion 10 on the container body 2 side.
  • the amount of protrusion of the tip of the scraper 15 with respect to the amount of protrusion of the protrusion 13B of the first concavo-convex portion 13 of the rotor is the ratio of the radius of the tip of the scraper 15 (R2) to the radius of the tip of the protrusion 13B (R1). [R2/R1] is preferably more than 1.005 and less than 2.0.
  • the number of scrapers 15 is preferably 2 to 500, more preferably 2 to 50, and even more preferably 2 to 10. Although the scraper 15 is provided in the grease manufacturing apparatus 1 shown in FIG. 2, it may be provided without the scraper 15 or may be provided intermittently.
  • the grease manufacturing apparatus 1 In order to manufacture the grease containing the urea thickener (B) by the grease manufacturing apparatus 1, the above-mentioned grease raw materials, the solution ⁇ and the solution ⁇ , are added to the solution introducing pipe 4A of the introducing portion 4 of the container body 2. 4B, and the rotor 3 is rotated at a high speed to produce a grease base material containing the urea thickener (B). Even if the additive (C) is added to the grease base material obtained in this way, the urea-based grease in the grease composition is satisfied so that the requirement (I) and the requirement (II) are satisfied.
  • the thickener can be miniaturized.
  • the shear rate applied to the grease raw material is preferably 10 2 s -1 or more, more preferably 10 3 s -1 or more, further preferably 10 4 s -1 or more, and , Usually 10 7 s ⁇ 1 or less.
  • the ratio (Max/Min) of the maximum shear rate (Max) and the minimum shear rate (Min) in shearing when the rotor 3 rotates at high speed is preferably 100 or less, more preferably 50 or less, and further preferably It is 10 or less.
  • the shear rate with respect to the mixed solution is as uniform as possible, the urea-based thickener and its precursor in the grease composition are easily miniaturized, and a more uniform grease structure is obtained.
  • the highest shear rate (Max) is the highest shear rate applied to the mixed solution
  • the lowest shear rate (Min) is the lowest shear rate applied to the mixed solution.
  • -Maximum shear rate (Max) (linear velocity of the tip of the convex portion 13B of the first concave-convex portion 13 of the rotor)/(tip of the convex portion 13B of the first concave-convex portion 13 of the rotor and the first inner circumference of the container body 2) Gap A1 of the convex portion of the first concave-convex portion 9 on the surface 6)
  • -Minimum shear rate (Min) (linear velocity of the recess 13A of the first uneven portion 13 of the rotor)/(recess 13A of the first uneven portion 13 of the rotor and the first inner peripheral surface 6 of the container body 2) Gap A2 of the concave portion of the one uneven portion 9)
  • the gap A1 and the gap A2 are as shown in
  • the grease manufacturing apparatus 1 includes the scraper 15, the grease attached to the inner peripheral surface of the container body 2 can be scraped off, so that lumps can be prevented from being generated during kneading, and the urea-based It is possible to continuously manufacture a grease having a finely-divided thickener in a short time. Further, the scraper 15 scrapes off the adhered grease to prevent the retained grease from becoming a resistance to the rotation of the rotor 3, so that the rotational torque of the rotor 3 can be reduced, and the drive torque can be reduced. The power consumption of the source can be reduced, and the continuous production of grease can be efficiently performed.
  • centrifugal force has an effect of discharging grease or a grease raw material in the downstream direction, and rotation.
  • the rotation torque of the child 3 can be reduced and the grease can be continuously manufactured.
  • a first uneven portion 13 of the rotor is provided on the outer peripheral surface of the rotor 3, and the first uneven portion 13 of the rotor is inclined with respect to the rotation shaft 12 of the rotor 3, and from the introduction portion 4 to the discharge portion 8.
  • the second concave-convex portion 14 of the rotor is inclined with respect to the rotation shaft 12 of the rotor 3, and has the ability to suppress the feed from the introduction section 4 to the discharge section 8.
  • the urea-based thickener (B) in the grease composition is finely divided so that a high shearing force can be imparted and the requirement (I) and further the requirement (II) can be satisfied even after the additive is compounded. Can be converted.
  • the first uneven portion 9 is formed on the first inner peripheral surface 6 of the container body 2 and is inclined in the opposite direction to the first uneven portion 13 of the rotor, the effect of the first uneven portion 13 of the rotor is obtained.
  • the urea-based thickener (B) in the grease composition can be miniaturized.
  • the second unevenness portion 10 is provided on the second inner peripheral surface 7 of the container body 2, and the second unevenness portion 14 of the rotor is provided on the outer peripheral surface of the rotor 3, so that the grease raw material is unnecessary more than necessary. Since it can be prevented from flowing out from the first inner peripheral surface 6 of the container body, even after the additive is compounded by giving a high shearing force to the solution to highly disperse the grease raw material,
  • the urea-based thickener (B) can be miniaturized so as to satisfy the requirement (II).
  • the grease composition of one aspect of the present invention may contain an additive (C) other than the component (B), which is blended with a general grease, within a range that does not impair the effects of the present invention.
  • the additive (C) include an antioxidant, a rust preventive, a dispersant, an extreme pressure agent, and a metal deactivator.
  • the additives (C) may be used alone or in combination of two or more kinds.
  • antioxidants examples include amine antioxidants such as diphenylamine compounds and naphthylamine compounds, and phenolic antioxidants such as monocyclic phenol compounds and polycyclic phenol compounds.
  • rust preventive for example, a carboxylic acid rust preventive such as alkenyl succinic acid polyhydric alcohol ester
  • examples include zinc stearate, thiadiazole and its derivatives, benzotriazole and its derivatives, and the like.
  • dispersant examples include ashless dispersants such as succinimide and boron succinimide.
  • Examples of the extreme pressure agent include thiocarbamic acids such as zinc dialkyldithiophosphate, molybdenum dialkyldithiophosphate, ashless dithiocarbamate, zinc dithiocarbamate, and molybdenum dithiocarbamate; sulfurized fats and oils, sulfurized olefins, polysulfides, thiophosphates, and thioterpenes. , Sulfur compounds such as dialkylthiodipyrionates; phosphoric acid esters such as tricresyl phosphate; phosphorous acid esters such as triphenyl phosphite.
  • Examples of the metal deactivator include benzotriazole compounds.
  • the content of the additive (C) is, independently of each other, usually 0.01 to 20% by mass, preferably 100% by mass based on the total amount (100% by mass) of the grease composition.
  • the amount is 0.01 to 15% by mass, more preferably 0.01 to 10% by mass, and further preferably 0.01 to 7% by mass.
  • the grease composition of the present invention is prepared by mixing the grease synthesized by the above method and containing the base oil (A) and the urea thickener (B) with various additives such as the additive (C). It can be manufactured. For example, it can be produced by mixing various additives such as the additive (C) and then stirring, or by mixing various additives such as the additive (C) while stirring the grease.
  • the mixing consistency at 25° C. of the grease composition of one embodiment of the present invention is preferably 180 to 350, more preferably 200 to 320, further preferably 220 to 310, and still more preferably 220 to 280.
  • the workability of the grease composition means the value measured at 25°C according to the ASTM D217 method.
  • the dropping point of the grease composition of one embodiment of the present invention is preferably 240°C or higher, more preferably 250°C or higher, even more preferably 255°C or higher, still more preferably 260°C or higher.
  • the dropping point of the grease composition means the value measured at 25° C. according to JIS K2208 8:2013.
  • the grease composition according to one aspect of the present invention has a bearing life (DN value: 200,000) in accordance with ASTM D 3336 of preferably 1200 hours or longer, more preferably 1500 hours or longer, still more preferably 1800 hours or longer, More preferably, it is 2000 hours or more.
  • the bearing life test conditions based on ASTM D 3336 are the same as those in Examples described later.
  • a bearing used under a high-speed rotation condition having a DN value of 1,000,000 or more is provided.
  • the grease composition of the present invention allows a bearing used under a high speed rotation condition of a DN value of 100,000 or more (preferably used under a high speed rotation condition of a DN value of 200,000 or more).
  • Bearing more preferably a bearing used under high speed rotation conditions with a DN value of 300,000 or more, even more preferably a bearing used under high speed rotation conditions with a DN value of 500,000 or more, even more preferably a DN value.
  • a lubrication method for lubricating a bearing used in a high speed rotation condition of 1 million or more is provided.
  • Example 1 (1) Synthesis of urea grease A base oil, poly ⁇ -olefin (PAO) heated to 70° C. (40° C. kinematic viscosity: 47 mm 2 /s, 100° C. kinematic viscosity: 7.8 mm 2 /s, viscosity index: 137) 92.04 parts by mass was added with 7.96 parts by mass of diphenylmethane-4,4'-diisocyanate (MDI) to prepare a solution ⁇ . Also, separately prepared poly ⁇ -olefin (PAO) heated to 70° C. (40° C. kinematic viscosity: 47 mm 2 /s, 100° C.
  • PAO poly ⁇ -olefin
  • kinematic viscosity 7.8 mm 2 /s, viscosity index: 137) 87.94 mass 2.01 parts by mass of cyclohexylamine and 10.05 parts by mass of stearylamine were added to the parts to prepare solution ⁇ .
  • the molar ratio of stearylamine to cyclohexylamine is 65/35. Then, using the grease manufacturing apparatus 1 shown in FIG. 1, the solution ⁇ heated to 70° C. is supplied from the solution introducing pipe 4A at a flow rate of 150 L/h, and the solution ⁇ heated to 70° C. is supplied from the solution introducing pipe 4B to a flow rate of 150 L/h.
  • R 1 and R 2 in the general formula (b1) are selected from a cyclohexyl group and a stearyl group (octadecyl group), and R 3 is diphenylmethylene. Corresponds to the compound that is the group.
  • Example 2 The base oil for preparing the solution ⁇ and the solution ⁇ was changed from PAO to mineral oil (40° C. kinematic viscosity: 138.0 mm 2 /s, 100° C. kinematic viscosity: 14.5 mm 2 /s, viscosity index: 104).
  • a grease composition (ii) was obtained in the same manner as in Example 1 except for the above. The content of each component in the grease composition (ii) is as shown in Table 1.
  • ⁇ Comparative Example 1> (1) Synthesis of urea grease The same solutions ⁇ and ⁇ prepared in Example 1 were used. Using the grease manufacturing apparatus shown in FIG. 3, the solution ⁇ heated to 70° C. was introduced into the container body from the solution introducing pipe at a flow rate of 504 L/h. Then, the solution ⁇ heated to 70° C. was introduced into the container main body containing the solution ⁇ at a flow rate of 144 L/h from the solution introducing pipe. After all the solution ⁇ was introduced into the container body, the stirring blade was rotated, the temperature was raised to 160° C. while continuing stirring, and the temperature was maintained for 1 hour to synthesize urea grease.
  • the maximum shear rate (Max) at this time was 42,000 s ⁇ 1 , and the ratio [Max/Min] of the maximum shear rate (Max) and the minimum shear rate (Min) was 1.03, and stirring was performed. It was (2) Preparation of grease composition After stirring the urea grease obtained in the above (1) (those discharged from the grease manufacturing apparatus shown in FIG. 3), it was cooled by natural cooling to obtain the additive (C).
  • a grease composition (iii) was obtained by adding 4,4-dinonyldiphenylamine, which is an antioxidant, and alkenylsuccinic acid polyhydric alcohol ester, which is a rust inhibitor.
  • the content of each component in the grease composition (iii) is as shown in Tables 1 and 2.
  • the particles (particles containing the urea thickener (B)) in the grease composition of the measuring cell were measured.
  • the arithmetic average particle diameter on an area basis was measured.
  • the 4,4-dinonyldiphenylamine and the alkenylsuccinic acid polyhydric alcohol ester used as the additive (C) are both liquids at room temperature (25° C.), so that the particles (urea-based particles) in the grease composition are It does not affect the measurement of the thickener (particles containing B)).
  • the "arithmetic mean particle size on an area basis” means a value obtained by arithmetically averaging the particle size distribution on an area basis.
  • the particle size distribution based on area is shown in FIG.
  • the particle size distribution on an area basis shows a frequency distribution of particle sizes in the whole particles to be measured, based on an area calculated from the particle size (specifically, a cross-sectional area of particles having the particle size). It is a thing.
  • the value obtained by arithmetically averaging the particle size distribution on the basis of area can be calculated by the following formula (1).
  • J means the division number of the particle size.
  • q(J) means a frequency distribution value (unit: %).
  • X(J) is a representative diameter (unit: ⁇ m) in the Jth particle diameter range.
  • the grease composition (i) prepared in Example 1 and the grease composition (iii) prepared in Comparative Example 1 were measured using a laser diffraction type particle size measuring device, and the particle size distribution on an area basis. Is shown in FIG. As is clear from the particle size distribution curve shown in FIG. 4, the particles containing the urea thickener (B) in the grease composition (i) prepared in Example 1 had the grease composition prepared in Comparative Example 1. It can be seen that, as compared with the particles containing the urea-based thickener (B) in the product (iii), the particles are clearly miniaturized.
  • Table 1 shows the evaluation results other than the specific surface area
  • Table 2 shows the evaluation results of the specific surface area
  • Comparative Examples 1 and 2 the particles containing the urea thickener (B) in the grease composition do not satisfy the requirement (I).
  • Comparative Example 1 the particles containing the urea thickener (B) in the grease composition do not satisfy the requirement (II). Therefore, when the particles containing the urea thickener (B) in the grease composition satisfy the above requirement (I) and further satisfy the above requirement (II), the effect of significantly extending the bearing life is achieved. You can see that it will be played.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Lubricants (AREA)
  • Sliding-Contact Bearings (AREA)
PCT/JP2020/003580 2019-01-31 2020-01-31 グリース組成物 WO2020158907A1 (ja)

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EP20749088.9A EP3919592A4 (en) 2019-01-31 2020-01-31 GREASE COMPOSITION
JP2020568622A JPWO2020158907A1 (ja) 2019-01-31 2020-01-31 グリース組成物
US17/423,252 US11746303B2 (en) 2019-01-31 2020-01-31 Grease composition
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